I'm posting this synth as the product of it serves as a staring material in the synthesis of the long-lived 2C-G-N. Also, those that are unlike me interested in MDxA synthesis can try this out and see how effective 1,4-naphthoquinone is as an oxygen donator in contrast to p-benzoquinone in Wacker process, involving donation of oxygen to the pi-bond of safrol. Advantage, as I see it, is that 1,4-naphthoquinone can bee prepared via
direct oxidation of common, non-suspicious, cheap naphthalene. Make it harder for DEA.
Place a solution of 120 g (1.2 mol) of pure chromium trioxide in 150 mL of 80 per cent aqueous acetic acid in a 2-litre three-necked flask, fitted with a thermometer, mechanical stirrer and 1-litre dropping funnel. Surround the flask by a mixture of ice and salt and, when the temperature has fallen to 0 Celsius, add a solution of 64 g (0.5 mol) of pure naphtalene in 600 mL of glacial acetic acid, with constant stirring, over a period of 2-3 hours while maintaining the internal temperature at 10-15°C. Continue the stirring overnight, during which time the reaction mixture and bath attain room T. Allow the dark green solution to stand for 3 days and stirr occasionally. Pour the reaction mixture into 5-6 litres of water, collect the crude naphtoquinone by suction filtration, wash with 200 mL of water and dry in a desiccator. Recrystallise from 500 mL of petroleum ether (b.p. 80-100°C). The yield of pure 1,4-naphtoquinone, m.p. 124-125°C, is 17 g (22%)